Environ. Sci. Technol.
1999, 33, 2095-2099
Potassium Persulfate as Oxidant in
Pressurized Hot Water
JUHANI KRONHOLM* AND
MARJA-LIISA RIEKKOLA
Laboratory of Analytical Chemistry, Department of Chemistry,
P.O. Box 55, University of Helsinki,
FIN-00014 Helsinki, Finland
Sub- and supercritical water oxidation are quite new
techniques for wastewater treatment. Temperatures must
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be high enough and reaction times long enough that
the organic compounds are completely oxidized into carbon
dioxide and water. The critical temperature and pressure
of water are 374 °C and 22.1 MPa. The primary aim of
the study was to determine whether potassium persulfate
is a feasible choice for oxidant in work clearly below
the critical temperature of water. Because potassium
Publication Date (Web): May 13, 1999 | doi: 10.1021/es9805977
persulfate is water soluble, it can be added directly to water
containing organic compounds. Simple equipment was
constructed for oxidation in high-temperature pressurized
water, and oxidation of phenol, 2,3-dichlorophenol, and
1-naphthol was carried out in aqueous environment at 75-
340 °C with potassium persulfate used as oxidant. The
pressure was adjusted to 25-45 MPa. The concentration
of the organic compounds was 1.0 mM, and that of the
oxidant was 1.0-10.0 mM. Study was made of the effects
of concentration, temperature, and reaction time on
oxidation efficiency. The removal percentages of phenol
were good even at 115 °C. Concentration of the oxidant
turned out to be a very important parameter. Also
temperature and reaction time had an effect on the
results. There were some problems arising from the
formation of rust and from blockage of the capillaries of
the equipment. However, the blockage could be prevented
with use of a precipitant collector.
Introduction
The theoretical possibilities of hot and pressurized water for
oxidation reactions have been known for more than a century,
but experimental and practical experiences were not widely
reported until the 1960s. The research on sub- and super-
critical water oxidation was first focused on temperatures
below the critical temperature and only later on the super-
critical state.
Today, wastewater treatment techniques exploiting the
oxidation power of hot pressurized water offer a promising
approach for converting organic substances into harmless
compounds such as water and carbon dioxide (1). The critical
temperature of water is 374.2 °C, and the critical pressure
22.1 MPa. If both or either of these values are smaller, water
is in the subcritical state. In the present work, where the
temperature range investigated was wide (75-340 °C), the
water is simply said to be pressurized and hot.
The physicochemical properties of water change in the
supercritical region. Above its critical temperature, water is
* Corresponding author phone: +358-9-191 40267; fax: +358-
9-191 40253; e-mail: juhani.kronholm@helsinki.fi.
10.1021/es9805977 CCC: $18.00  1999 American Chemical Society
Published on Web 05/13/1999
like a dense gas and behaves like a fluid. Its density and
viscosity are reduced, and the Brownian diffusion is increased
(2, 3). The dielectric constant and extent of hydrogen bonding
are also reduced (4-7), resulting in increased solubility of
organic compounds and gases and decreased solubility of
electrolytes (8). As the temperature in the subcritical region
is raised, the properties of the water approach those in the
supercritical region.
For treatment purposes, it is not necessary to raise the
temperature up to 374 °C or further if complete destruction
of the organic compounds can be achieved at temperatures
below 374 °C. The main incentive for working below the
critical temperature is to save energy. With large-scale systems
consuming large amounts of energy, energy costs become
of critical importance. In addition, inorganic compounds
are precipitated at temperatures higher than the critical
temperature of water, so that working below this temperature
may prevent the formation of insoluble matter and blockage
of the capillaries of the equipment.
To ensure the effective oxidation of organic pollutants
into water and carbon dioxide, it is usual to add an oxidant
to the reaction chamber. Oxygen and hydrogen peroxide have
been widely used with excellent results. For example, pulp
and paper mill sludges have been successfully purified (9,
10), and wastewaters containing phenol have been effectively
treated under supercritical conditions (11-13). Potassium
persulfate, which was the oxidant used in this study, is not
a common choice but was of interest to us as an effective
and exothermic reactant. Besides oxidants, catalysts (for
example, transition metal salts such as CuO, ZnO, MnO2,
and V2O5) have been used under supercritical conditions to
lower the activation energy of the reaction and thus enhance
the destruction rate (14-16). Catalysts have also been used
at temperatures clearly below the supercritical temperature
to destroy phenolic compounds (17-20).
The primary aim of our study was to evaluate the feasibility
of using potassium persulfate as oxidant at temperatures
clearly below the critical temperature of water. Inorganic
compounds are a problem in work in supercritical conditions,
and at temperatures clearly below the critical temperature
of water, it may be possible to prevent the precipitation of
inorganic compounds and the blockage of capillaries. A
second aim of the study was to construct simple laboratory
equipment allowing the destruction of organic compounds
reliably and safely at high temperatures and under high
pressures. Phenol, 2,3-dichlorophenol, and 1-naphthol were
chosen as the organic contaminants because all are common
aromatic pollutants and information is available on the
destruction efficiencies of closely related compounds in
pressurized hot water.
Experimental Section
Materials. Phenol (E. Merck, Darmstadt), 2,3-dichlorophenol
(Fluka AG, Buchs SG), and 1-naphthol (E. Merck, Darmstadt)
were chosen as the model contaminants. Concentration of
each compound in water (distilled and deionized) was 1.0
mM. The water containing the contaminants is afterward
simply referred to as the wastewater. Potassium persulfate
(E. Merck, Darmstad) was added to the wastewater as an
oxidant (c ) 1.0-10.0 mM). Two internal standards were
used in sample analysis: m-cresol (Fluka AG, Buchs SG) and
hexachlorobenzene (Sigma-Aldrich). Dichloromethane (Lab-
Scan, Analytical Sciences, HPLC grade) was used as the
solvent in extraction.
Instrumentation. Figure 1 shows a simplified view of the
subcritical water oxidation equipment. All the capillaries (1/
VOL. 33, NO. 12, 1999 / ENVIRONMENTAL SCIENCE & TECHNOLOGY 9 2095
 FIGURE 1. Equipment constructed for oxidation in pressurized hot
water. The precipitant collector is described in detail in the area
bounded with a dashed line.

16 in. o.d.), the reaction chamber (Keystone Scientific

extraction chamber, V ) 5.0 mL), and the precipitant collector
(V ) 2.0 mL) were made of stainless steel. One high-pressure
pump (Perkin-Elmer Series 1) and a heating oven (Carlo Erba
Fractovap model G1) were used in this study, an ice-bath
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FIGURE 2. Removal percentages of phenol (c ) 1.0 mM) at four
temperatures (115, 195, 275, and 340 °C) and three concentrations
of potassium persulfate. Average reaction times were 1.4-2.5 min,

was added to cool the hot effluent, and a pressure regulator and the average pressure was 33-38 MPa (exact values in Table
(needle valve) was installed to adjust the pressure. 1).
A Hewlett-Packard model 5890 gas chromatograph and
a model 5989A mass spectrometer (EI, 70 eV) were employed
to analyze the compounds left in the effluent. The analytical
column of the gas chromatograph was a polar Nordion NB
351 (20.0 m, 0.2 mm i.d., 0.2 µm). The precolumn (2.5 m, 0.53
Publication Date (Web): May 13, 1999 | doi: 10.1021/es9805977

mm i.d.) attached in front of the analytical column was

deactivated with DPTMDS (1,3-diphenyl-1,1,3,3-trimethyl-
silazane). The injection mode was on-column.
Procedure. Most of the experiments were carried out with
phenol as the organic pollutant, and a few additional
experiments were carried out with 2,3-dichlorophenol and
1-naphthol. The wastewater, containing the added oxidant,
was pumped into the heated reaction chamber by means of
a high-pressure pump. In some arrangements, a precipitant
collector was installed before the reaction chamber to prevent
blockage of the capillaries. The flow rates of the wastewater
feed were adjusted to 1.9-5.4 mL/min. In this text, we prefer
the expression reaction time to flow rate because flow rate FIGURE 3. Removal percentages of phenol (c ) 1.0 mM) at four
is strictly related to the high-pressure pump, whereas the temperatures (75, 115, 250, and 340 °C) and three concentrations of
reaction time expresses the time the aqueous waste is potassium persulfate. Average reaction times were 1.2-1.5 min,
subjected to certain reaction conditions. Pressure and flow and the average pressure was 32-43 MPa (exact values in Table
rates fluctuated a little during sample collection (by about 1).
5 MPa on average), and the values given are averages of the
minimum and maximum values. However, pressure was kept
high enough to maintain water in liquid state.
Three effluent samples were collected under each set of
conditions (experiments with phenol). Each point in the
graphical presentations (Figures 2-4) represents an average
removal percentage of phenol. The relative standard devia-
tions of the replicates are noted in Table 1. After the samples
were collected at the outlet of the capillary, they were
extracted with dichloromethane (4 × 2.0 mL) and finally
concentrated to 2.0 mL by gentle nitrogen evaporation. Two
internal standards were used: one (m-cresol, added before
the extraction) to calculate the removal percentages of the
organic pollutants and the other (hexachlorobenzene, added
after the extraction) to calculate the extraction efficiencies.
The removal percentage entered in the tables is the amount
of compound that was destroyed under the conditions in
question. FIGURE 4. Removal percentages of phenol (c ) 1.0 mM) as a function
This was calculated as follows: of potassium persulfate concentration (1.0, 2.0, 5.0, and 10.0 mM)

[ ]
at four temperatures. Average reaction times were 1.2-1.5 min,
std1a and the pressure was 32-43 MPa (exact values in Table 1).
X1a
removal percentage ) 100 × 1 -
std1b is the peak area of the internal standard (m-cresol) added to
X1b the collected sample before extraction, X1a is the peak area
of the analyte in the reference sample, and X1b is the peak
where std1a is the peak area of the internal standard (m- area of the analyte in the collected sample. The reference
cresol) added to the reference sample before extraction, std1b sample was a sample treated at room temperature.

2096 9 ENVIRONMENTAL SCIENCE & TECHNOLOGY / VOL. 33, NO. 12, 1999
 TABLE 1. Oxidation Efficiencies for Phenol (c ) 1.0 mM) at Various Temperatures and Oxidant (Potassium Persulfate)
Concentrationsa
temp oxidant concn reaction time pressure removal RSD precipitant collector
exp (°C) (mM) (min) (MPa) (%) (%) in use
1 75 1.0 1.4 35 0 X yes
2 75 2.0 1.3 32 10.4 141.4 yes
3 75 5.0 1.4 37 3.3 173.2 yes
4 75 10.0 1.5 43 29.1 83.6 yes
5 115 no oxidant 1.4 33 12.5 86.9 no
6 115 1.0 2.3 35 23.9 89.7 no
7 115 1.0 1.4 37 7.3 105.9 yes
8 115 2.0 1.2 35 7.4 87.2 yes
9 115 5.0 1.4 40 99.6 0.1 yes
10 115 10.0 2.3 37 99.7 0.1 no
11 115 10.0 1.5 40 99.8 0.2 yes
12 195 no oxidant 2.4 34 8.1 125.9 no
13 195 1.0 2.3 38 59.6 22.0 no
14 195 10.0 2.3 35 99.9 0.0 no
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15 250 1.0 1.5 40 41.2 6.6 yes

16 250 2.0 1.3 40 95.5 0.2 yes
17 250 5.0 1.5 38 98.9 0.1 yes
18 250 10.0 1.4 40 99.5 0.1 yes
19 275 no oxidant 2.4 35 0 X no
20 275 1.0 2.4 33 62.9 10.1 no
21 275 10.0 2.4 37 99.3 0.1 no
22 340 no oxidant 2.3 37 0 X no
Publication Date (Web): May 13, 1999 | doi: 10.1021/es9805977

23 340 1.0 2.2 33 65.4 2.8 no

24 340 1.0 1.5 35 40.9 9.7 yes
25 340 2.0 1.2 40 88.7 3.4 yes
26 340 5.0 1.5 38 97.0 0.3 yes
27 340 10.0 2.5 37 99.3 0.0 no
28 340 10.0 1.5 42 97.4 0.3 yes
a Reaction times, pressures, and removal percentages are averages (n ) 3). The reaction volume was 7.0 mL when the precipatant collector

was in use and 5.0 mL when it was not. An X means that only two replicates were performed under each set of conditions and that no RSD is
included.

concentration of the oxidant to obtain good results (see

FIGURE 5. Some oxidation reactions of phenol, 2,3-dichlorophenol,
and 1-naphthol. In practice, inorganic compounds are present as
salts or ions in aqueous environment. The reactions in the figure
are highly simplified, and no intermediate reaction products are
presented.
Results and Discussion
Figures 2-4 present the oxidation efficiencies for phenol at
different temperatures and different concentrations of
oxidant. Table 1 gives the numerical and exact information
on which the figures are based. The theoretical ratio of oxidant
to phenol needed to convert all the phenol into carbon dioxide
and water is 7/4 (see Figure 5). Note: The reactions presented
in Figure 5 are theoretical because no intermediate products
are included, and only the initial and final products are shown;
the main reason for presenting the figure is to indicate the
stoichiometry of the reactions and thus the equivalent
amounts of oxidant needed for the oxidation process. The
ratio 7/4 means that a potassium persulfate concentration
of 2.0 mM should be stoichiometrically high enough to oxidize
all the phenol (c ) 1.0 mM).
A good removal percentage was obtained when the
concentration of potassium persulfate was 2.0 mM and the
temperature at least 250 °C (see Figures 3 and 4). When the
oxidant concentration was increased to 5.0 mM, results were
excellent even at temperatures as low as 115 °C. A temperature
of 75 °C was clearly too low, and 1.0 mM was too low a
Figures 2-4). It was evident that by increasing the concen-
tration of potassium persulfate from 2.0 to 5.0 mM and further
up to 10.0 mM the oxidation efficiency was improved.
Potassium persulfate is an inorganic salt, soluble in water
(5.3 g/100 mL, 20 °C) (21) that begins to react strongly and
release oxygen when the temperature is raised to 100 °C. The
reaction is strongly exothermic.
Possibly not all the oxidant present is available for
oxidizing phenol since there will always be small amounts
of impurities in the water even though the water is distilled
and deionized and all the reagents are of high purity. There
may also be a number of side reactions occurring simulta-
neously before the final products appear, and this could lead
to increased oxidant consumption. When the concentration
of potassium persulfate was below the stoichiometric re-
quirement (0-1.0 mM), the results were poor even when the
temperature was raised to 340 °C. The results demonstrate
the importance of the stoichiometric requirement of the
oxidant.
The temperature, reaction time, and pressure employed
are of great importance. The temperature must be high
enough to increase the exothermic energy to values able to
break down the chemical bonds and to produce activation
energies high enough for the desired reactions. In some cases,
the removal percentages of phenol were a little lower when
the temperature was raised. The real reason for this is unclear,
but these observations are statistically nonsignificant. Water
has itself some ability to work as an oxidant (22), but it is not
clear why the oxidation efficiency decreased with increasing
temperature when no oxidant was used (Figure 2). In theory,
pressure may influence the results through altering the
density of water, so that an increase in pressure (at constant
temperature) increases the density and the number of
molecules colliding. It has been observed in another study

VOL. 33, NO. 12, 1999 / ENVIRONMENTAL SCIENCE & TECHNOLOGY 9 2097

TABLE 2. Removal Percentages of Phenol, 2,3-Dichlorophenol,
and 1-Naphthola
temp reaction time
exp compound (°C) (min)
29 phenol 250 3.3
30 phenol 340 5.0
31 2,3-dichlorophenol 250 5.0
32 2,3-dichlorophenol 340 5.0
33 1-naphthol 250 5.0
34 1-naphthol 340 5.0
a Concentration of each compound was 1.0 mM, and concentration
of the oxidant (potassium persulfate) was 10.0 mM. The pressure was
≈45 MPa. Relative standard deviations are not included because only
one effluent sample was collected under each set of conditions.
(23), where results under pressures of 188 and 278 atm were
compared, that pressure influences the destruction efficien-
cies of phenol clearly at 360-440 °C, but the influence was
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almost negligible at the temperatures used in our study (at
temperatures below 340 °C and where water was still in liquid
state). This is why we believe that the differences in pressure
in our study do not have a remarkable effect on destruction
efficiencies. The pressure effects on rate for elementary
reaction steps are pressure dependent according to transition
Publication Date (Web): May 13, 1999 | doi: 10.1021/es9805977
state theory. The pressure effects on rate constant are
governed by the relationship
[ ∂P ]
∂ ln kx
T
)
-∆V+
RT
where ∆V+ is the activation volume and kx is the rate constant.
Some additional studies were carried out with 2,3-dichloro-
phenol and 1-naphthol (see Table 2) to determine whether
these compounds could be removed as effectively as phenol.
Only one effluent sample was collected under each set of
conditions, so relative standard deviations are not included
in the table. Concentrations of these compounds were 1.0
mM, while the concentration of potassium persulfate was
kept constant at 10.0 mM. The removal percentages of these
compounds were good too, although the reaction time was
relatively long (3.3-5.0 min) because the precipitant collector
was not used and there were problems in increasing the flow
rate due to blockage of the capillaries.
Phenol, 2,3-dichlorophenol, and naphthol were collected
quantitatively; in other words, no compounds were found in
the capillaries or in the reaction chamber when they were
eluted with dichloromethane after the oxidation process. It
can be concluded that the oxidation process and not the loss
of these compounds was responsible for the high removal
percentages. We conclude that the removal percentages of
phenol, 2,3-dichlorophenol, and 1-naphthol are very good
when the parameters (oxidant concentration, temperature,
and reaction time) are correctly adjusted. Raising the
temperature up to 340 °C is not necessary to achieve good
results if the concentration of oxidant is 5.0 mM or higher
and the reaction time at least 1.5 min.
Catalytic oxidation of phenol has been studied on many
occasions. Temperatures between 100 and 200 °C have been
widely used, and the reaction times required to oxidize phenol
effectively have usually ranged between 5 min and 1 h (17,
18, 20, 24). Faster reaction times have been achieved at
temperatures lower than 100 °C, but the catalysts were
heterogeneous (19). We found no need to employ a separate
catalyst because potassium persulfate worked effectively as
oxidant.
Water is highly corrosive at high temperatures (25), and
at 115-340 °C, the samples collected at the outlet of the
equipment were dirty (the effluent was reddish brown).
Another source of color and also of inorganic matter is that
2098 9 ENVIRONMENTAL SCIENCE & TECHNOLOGY / VOL. 33, NO. 12, 1999
potassium persulfate is reduced in the oxidation process,
and some potassium and sulfur compounds are released.
The color was strongest at temperatures of 195-275 °C and
removal got lighter again at 340 °C. Investigations by others suggest
% that corrosion in oxidation processes in water at high
temperatures may be strongest below the critical temperature
99.5
(26, 27). In addition to this, we observed that the reddish
97.6
98.4 brown color intensified when the concentration of the oxidant
99.6 was increased. Corrosion and color formation may be heavily
94.4 dependent on the oxidant, and our observations do not apply
96.3 beyond systems in which potassium persulfate is the oxidant.
Several investigations have shown that ordinary stainless steel
is not the best choice for work with water at high temper-
atures. Better choices may be Inconel 600, Inconel 625, and
Hastelloy C-276 (28, 29). In preliminary investigations that
we carried out with Inconel 600, rust formation was clearly
less, and the samples were cleaner.
Rust formation and the precipitation of inorganic com-
pounds caused some problems when the precipitant collector
was not connected. To avoid blockage of the capillaries, we
occasionally adjusted the pressure regulator so that the flow
rate was momentarily increased and the pressure decreased.
After this, the pressure regulator was readjusted to return to
the original pressure. In some of the experiments the
precipitant collector was installed in front of the reaction
chamber (see Table 1) allowing the inorganic matter to be
collected at the bottom of the collector. This arrangement
prevented the capillaries from getting blocked, and there
was no need for pressure adjustments. We would conclude
that, even when the reaction temperature is clearly below
the critical temperature of water, a precipitant collector needs
to be used to ensure constant flow. The diameter of our
capillaries was small (1/16 in. o.d.) and use of capillaries of
larger diameter, 1/8 in. o.d., for example, might have reduced
the problems with inorganic compounds.
Outside of the problems noted, the organic pollutants
were effectively destroyed and no hazards arose. Despite
rapid drops in pressure, there were no leaks in the joints of
the capillaries. Further investigations will be made with
materials more resistant to corrosion than stainless steel and
with a two- or three-pump system delivering the organic
matter and oxidant to the reaction chamber separately. Also,
capillaries with larger diameters will be used to prevent
blockage. Further investigations with potassium persulfate
as oxidant should be made to determine the effects of
temperatures between 340 and 400 °C, an increase in the
potassium persulfate concentration beyond 10.0 mM, and
the use of a wider range of reaction times. It would also be
worth trying to improve the oxidation efficiency by adding
potassium persulfate in hydrogen peroxide.
Acknowledgments
Financial support for this study was provided by the Maj &
Tor Nessling Foundation and the Jenny & Antti Wihuri
Foundation.
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Received for review June 12, 1998. Revised manuscript re-
ceived January 22, 1999. Accepted March 26, 1999.
ES9805977
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